EP3374763B1 - Vorrichtung und verfahren zur bestimmung der feuchtigkeit einer probe - Google Patents

Vorrichtung und verfahren zur bestimmung der feuchtigkeit einer probe Download PDF

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Publication number
EP3374763B1
EP3374763B1 EP16794312.5A EP16794312A EP3374763B1 EP 3374763 B1 EP3374763 B1 EP 3374763B1 EP 16794312 A EP16794312 A EP 16794312A EP 3374763 B1 EP3374763 B1 EP 3374763B1
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EP
European Patent Office
Prior art keywords
sample
chamber
measuring
moisture
sensor
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
EP16794312.5A
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German (de)
English (en)
French (fr)
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EP3374763A1 (de
Inventor
Kay Fremuth
Tobias Nabbefeld
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Anton Paar TorqueTec GmbH
Original Assignee
Brabender Messtechnik GmbH and Co KG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
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Publication of EP3374763A1 publication Critical patent/EP3374763A1/de
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Publication of EP3374763B1 publication Critical patent/EP3374763B1/de
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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N19/00—Investigating materials by mechanical methods
    • G01N19/10—Measuring moisture content, e.g. by measuring change in length of hygroscopic filament; Hygrometers
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00—Investigating or analyzing materials by the use of thermal means
    • G01N25/56—Investigating or analyzing materials by the use of thermal means by investigating moisture content
    • G01N25/66—Investigating or analyzing materials by the use of thermal means by investigating moisture content by investigating dew-point
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/048—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance for determining moisture content of the material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00—Indexing codes associated with group G01N29/00
    • G01N2291/02—Indexing codes associated with the analysed material
    • G01N2291/021—Gases
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/44—Resins; Plastics; Rubber; Leather
    • G01N33/442—Resins; Plastics

Definitions

  • the invention relates to a device for determining the humidity of a sample containing a solid mixture, with (i) at least one sample chamber for receiving the sample, (ii) at least one sensor for measuring a parameter of a gas mixture surrounding the sample and (iii) a determination device for determination the moisture of the sample from the at least one parameter.
  • the invention further relates to a corresponding method for determining the moisture of a sample containing a solid mixture.
  • Such a device is used as a device for determining the humidity of bulk materials from the DD 155 115 A1 known.
  • this device there is a space, for example in a screw conveyor for conveying the bulk material, in which the bulk material itself and a gas space above this bulk material are located.
  • the device has a temperature sensor as well as a dew point sensor, which measure the parameters temperature and dew point of the gas mixture located in the gas space.
  • the output signals of these sensors are fed to a determination device for determining the humidity by converting and linking the output signals, taking into account a dew point-temperature curve, which in turn outputs an output signal for display or control.
  • the accuracy of the determination of the moisture content of the bulk material described in this publication is relatively low, not least because one does not wait for an equilibrium in the water content between the gas and the solid mixture to be established.
  • the pamphlet EP 0 520 472 A2 describes a device for determining the moisture of a sample containing a solid mixture, with at least one sample chamber for receiving the sample, at least one sensor for measuring a parameter of a gas mixture surrounding the sample, a determination device for determining the moisture of the sample from the at least one parameter and one Measuring chamber in addition to the sample chamber.
  • the invention is based on the object of specifying a device and a corresponding method for determining the moisture content of a sample which enable the moisture content of samples to be determined quickly and accurately without using consumable material.
  • the device for determining the humidity of a sample containing a solid mixture with the features mentioned in the preamble of claim 1, it is provided that the device has an evacuable measuring chamber which can be separated fluidically from the at least one sample chamber and can be connected to the sample chamber the at least one sensor is set up to measure the parameter of the gas mixture in the measuring chamber.
  • the device is preferred a device for determining the humidity of a bulk material sample or another sample consisting of a solid mixture.
  • the humidity of the sample is determined by means of the device as follows: First, the sample is brought into the sample chamber and, if necessary, prepared there such that the gas mixture surrounding the sample is formed in the desired manner in the sample chamber. Then the sample chamber is fluidically connected to the previously evacuated measuring chamber, so that part of the gas mixture surrounding the sample flows out of the sample chamber into the measuring chamber, where the measurement of the at least one parameter of the gas mixture takes place. The moisture of the sample located in the measuring chamber is then determined by means of the determination device from the at least one measured parameter. A subsequent fluidic connection of the evacuated measuring chamber with the sample chamber or one of the sample chambers results in an expansion of the gas mixture from the sample chamber into the measuring chamber The operating point required for the exact measurement is located on the dew point curve. The evacuation results in a dew point temperature T dew point of -20 ° C., for example. The volume of the interior of the measuring chamber is preferably approximately three liters. The sample chamber (s) usually has / have a significantly smaller internal volume.
  • the device has at least one shut-off valve, such as a valve or a slide, via which the at least one sample chamber can optionally be fluidically connected to the measuring chamber or separated from the measuring chamber.
  • a shut-off valve such as a valve or a slide
  • the device has at least one heater for heating the sample in the at least one sample chamber.
  • the heating temperature is there preferably above 100 ° C, particularly preferably in the range of 200 ° C, i.e. about 150 ° C ⁇ T H ⁇ 250 ° C.
  • the measuring chamber (at least at the time of the measurement) preferably has a significantly lower temperature T M , that is to say T M ⁇ T H , preferably room temperature. As a rule, however, measurement temperatures T M of up to 60 ° C. are also possible.
  • T M is to say T M ⁇ T H , preferably room temperature.
  • measurement temperatures T M of up to 60 ° C. are also possible.
  • the use of measuring and sample chambers has the advantage that the sensor or the sensors do not have to be baked out, since they are attached in or on the unheated measuring chamber.
  • the measuring chamber can of course be evacuated with an external vacuum pump.
  • the device has its own pump for optionally evacuating the measuring chamber. It is usually completely sufficient if the pump is able to pump out / empty the measuring chamber down to the rough vacuum range, that is to say in the range of a few hPa or mbar residual gas pressure (for example 10 hPa).
  • the pump is preferably fluidically connected to the measuring chamber or separated from the measuring chamber via a shut-off valve, such as a valve or a slide.
  • several sample chambers are provided.
  • several samples can be heated in parallel and the corresponding parameters can be measured at a relatively high measuring rate, that is, a high repetition rate of the measurements.
  • sensors are provided. These sensors preferably measure different parameters.
  • One of the sensors is advantageously a temperature sensor.
  • the determination device can then determine the moisture of the sample from the parameters of these sensors.
  • the senor or at least one of the sensors is a dew point sensor.
  • the result is a device whose basic measuring principle is somewhat similar to the measuring principle mentioned at the beginning of the DD 155 115 A1 having.
  • a significantly higher accuracy can be achieved when determining the sample moisture.
  • the dew point sensor determines the dew point temperature with the aid of a capacitive sensor element.
  • a sensor element can be a sensor element based on a metal-ceramic or a polymer sensor element. The moisture-dependent capacity and the temperature of the gas are measured in a calibration process.
  • the dew point sensor has a dew point mirror as a sensor element. This can also be used as a reference instrument for absolute humidity.
  • the device furthermore has a measuring, control and / or regulating device which is connected to the at least one sensor for signaling purposes and which also forms the determination device.
  • the measuring, control and / or regulating device is preferably also connected in terms of signaling to the at least one heater and / or to the shut-off valve or valves.
  • the entire process of moisture determination is controlled or regulated by means of the measuring control and / or regulating device and, at the end, the moisture of the sample is determined from the measured parameter or the measured parameters.
  • the device also has at least one fluid circulation system in which the measuring chamber is connected in terms of flow.
  • this fluid circulation system for example, the residual moisture in the measuring system can be evenly distributed.
  • the at least one sample chamber in the at least one fluid circulation system can optionally be interconnected or permanently interconnected.
  • the gas mixture surrounding the sample can be introduced into the measuring chamber quickly and in a controlled manner.
  • the Fig. 1 shows a device 10 for determining the moisture of a sample comprising a solid mixture (sample not shown).
  • the main components of the device are a measuring chamber 12 and a sample chamber 14 for receiving the sample.
  • the device 10 can of course also have several such sample chambers 14, but since this is only a schematic representation, only one of these sample chambers 14 is shown.
  • the volume of the interior of the measuring chamber 12 is preferably approximately 3 liters.
  • the sample chamber (s) 14 usually has / have a significantly smaller internal volume.
  • the sample chamber 14 is fluidically connected to the measuring chamber 12 via a fluid connection element 16 designed as a connecting tube or in fluid communication.
  • a shut-off fitting 18 designed as a valve is connected in the fluid connection element 16.
  • the device also has a pump 20 for optionally evacuating the measuring chamber 12.
  • the pump 20 is also fluidically connected to the measuring chamber 12 via a fluid connection element 22 configured as a connecting tube or in fluid communication.
  • a shut-off fitting 24 designed as a valve is also connected in this fluid connection element 22.
  • two sensors 26, 28 for measuring parameters of a gas mixture located in the interior of the measuring chamber are fastened.
  • One of the sensors is a dew point sensor 26, the other a temperature sensor 28.
  • a heater 30 is attached to the sample chamber 14 for heating the interior of the sample chamber 14, that is to say in particular the sample located there.
  • a temperature sensor 32 is also attached to this heater (or alternatively to the sample chamber).
  • the device 10 also has a measuring, control and / or regulating device 34 connected to the sensors 26, 28, the at least one heater 30 and the temperature sensor 32, the pump 20 and the shut-off fittings 18, 24 for signaling purposes.
  • the named components 18, 20, 24, 30 can be controlled by the measuring, control and / or regulating device 34 and the named sensors and the measuring sensors 26, 28, 32 can be read out by the measuring, control and / or regulating device 34.
  • the result is the following function:
  • the sample to be measured with a known density is weighed and placed in the sample chamber 14.
  • the fitting 18 between the sample chamber 14 and the measuring chamber 12 is closed.
  • the heater 30 heats the sample chamber 14 and the sample located therein to a desired temperature (for example about 200 ° C.).
  • the valve 24 between the pump 20 and the measuring chamber 12 is open and the measuring chamber 12 is pumped out by means of the pump 20. After a few minutes (depending on the size of the measuring chamber 12 and the power of the pump 20), a stable negative pressure and thus also a corresponding dew point (i.e. a corresponding dew point temperature) has set in the measuring chamber 12 and the sample chamber 14 with the sample located therein reaches a constant temperature for the measurement.
  • shut-off valve 24 between the pump 20 and the measuring chamber 12 is closed and then the sample chamber 14 is fluidically connected to the empty measuring chamber 12 by opening the shut-off valve 18, so that part of the gas mixture surrounding the sample from the sample chamber 14 into the measuring chamber 12 flows, where the measurement of the parameter of this gas mixture takes place.
  • the water from the sample passes into the gas phase due to the increased measuring temperature and the now reduced vapor pressure and now changes the dew point in the measuring chamber 12. After a while, the dew point is constant.
  • the moisture of the sample located in the measuring chamber 14 is determined from the measured parameters by means of a determination device 36 formed by the measuring, control and / or regulating device 34. With the measured temperature and the dew point, the amount of water present per unit volume can be calculated. Since the volume in the measuring range and the volume of the sample (via weight and density) are known, the absolute amount of water in the system can be calculated and compared with the original weight of the sample.
  • the fluid system of the device 10 can now be aerated and the next sample can be measured. Since the sample chamber 14 is still hot, further sample chambers 14 can be connected to the measuring chamber 12 via connecting elements 16 and fittings 18. This makes it possible to take measurements at shorter intervals.
  • the dew point is determined before the actual measurement and the amount of water per unit volume is calculated.
  • the absolute amount of water that is in the air of the sample chamber 14 and the connected connecting element 16 is subtracted from the absolute amount of water in the system calculated at the end of the measurement.
  • the moisture in a solid mixture sample can be reliably determined without consumable material down to the range of a few ppm.
  • a moisture determination with such accuracy is desirable, for example, when processing solid mixture samples such as plastic granulates.
  • the device 10 shown is designed as a mobile moisture measuring device, even as a portable moisture measuring device.
  • FIGS. 2 to 5 show a further embodiment of the device 10 for determining the moisture of a sample containing a solid mixture. Since those in the Figures 2 to 5 The device 10 shown essentially corresponds to that in FIG Fig. 1 corresponds to the device 10 shown, only the differences will be discussed here.
  • the device shown has a fluid circulation system 38 in which the measuring chamber 12 and the pump 20 are permanently connected in terms of flow, while the sample chamber 14 can optionally be connected in this fluid circulation system 38.
  • the sample chamber 14 is connected in a line section 40, to which the fluid circulation system 38 has a bypass 42 connected in parallel.
  • the sample chamber 14 is surrounded in the line section 40 by two shut-off fittings 44, 46 and the bypass also has a shut-off fitting 48.
  • the line section 40 or the bypass 42 can optionally be integrated into the circulatory system 38 via these fittings 44, 46, 48.
  • These shut-off valves 44, 46, 48 also take on the function of the in Fig. 1 shown device known shut-off valve 24.
  • the device 10 has ventilation and / or venting valves or other fittings 50, 52, via which the circulatory system 38 can be ventilated and / or vented. All of the fittings 18, 44, 46, 48, 50, 52 can be designed as valves, for example, and are preferably activated by the measuring, control and / or regulating device 34.
  • Fig. 2 shows the first of these phases, namely the pumping process.
  • the measuring chamber 12 is evacuated by means of the pump 20.
  • the sample chamber 14 is separated from the rest of the circulatory system 38 by the two shut-off valves 44, 46 which are positioned directly in front of and behind the sample chamber 14. This means that the sample can already be baked out in this phase.
  • the gas can be pumped out of the measuring chamber 12 past the sample chamber 14 via the bypass 42 and is released into the environment via the fitting 50 (arrow 54).
  • the pumping process is ended as soon as a specified dew point temperature (typically ⁇ -20 ° C) or, if a different sensor is selected, a specified negative pressure (typically approx. 10 mbar absolute) is reached.
  • a specified dew point temperature typically ⁇ -20 ° C
  • a specified negative pressure typically approx. 10 mbar absolute
  • Fig. 3 shows the second of the phases, namely a calming phase.
  • the circulatory system 38 is closed to the outside.
  • the sample chamber 14 is also still separated from the measuring chamber 12 and continues to be heated.
  • the pump 20 allows the residual gas to circulate in the system 38 in this phase.
  • This circulation of the residual gas firstly leads to the residual moisture which is still in the system 38 being evenly distributed.
  • the relatively sluggish dew point temperature sensor 26 and the relatively sluggish temperature sensor 28 reach a state of equilibrium and thus a stable value. This is important because the residual moisture remaining in the system is subtracted from the calculated moisture content of the sample at the end of the actual measurement process.
  • the calming phase is ended after a specified time (typically approx. 2 minutes).
  • Fig. 4 shows the third of the phases, namely the actual measurement phase.
  • the bypass 42 is shut off by the shut-off valve 48.
  • the two shut-off valves 44, 46 in front of and behind the sample chamber 14 are opened.
  • the pump 20 ensures that the gas mixture surrounding the sample circulates from the sample chamber 14 in the system 38 and thus the moisture from the sample is quickly and evenly distributed in the system 38.
  • the sample continues to be baked out.
  • the measuring phase or the measuring process can be ended as soon as the value calculated from the dew point temperature and gas temperature for the amount of water (moisture) contained in the gas is constant.
  • the Fig. 5 finally shows the fourth of the phases, namely a rinsing process in preparation for the next measurement.
  • a rinsing process in preparation for the next measurement.
  • the pump 20 ensures a flow of surrounding air through the complete system 38, in which there is now again atmospheric pressure (arrows 54, 56). Both the flow through the line section 40 with the sample chamber 14 and through the bypass 42 are provided. The sample chamber 14 is no longer heated. The air flow also ensures a faster cooling process.

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  • Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Investigating Or Analyzing Materials Using Thermal Means (AREA)
EP16794312.5A 2015-11-09 2016-11-09 Vorrichtung und verfahren zur bestimmung der feuchtigkeit einer probe Active EP3374763B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102015119267.5A DE102015119267A1 (de) 2015-11-09 2015-11-09 Vorrichtung und Verfahren zur Bestimmung der Feuchtigkeit einer Probe
PCT/EP2016/077169 WO2017081099A1 (de) 2015-11-09 2016-11-09 Vorrichtung und verfahren zur bestimmung der feuchtigkeit einer probe

Publications (2)

Publication Number Publication Date
EP3374763A1 EP3374763A1 (de) 2018-09-19
EP3374763B1 true EP3374763B1 (de) 2021-03-17

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Application Number Title Priority Date Filing Date
EP16794312.5A Active EP3374763B1 (de) 2015-11-09 2016-11-09 Vorrichtung und verfahren zur bestimmung der feuchtigkeit einer probe

Country Status (7)

Country Link
US (1) US10852226B2 (enExample)
EP (1) EP3374763B1 (enExample)
JP (1) JP6933655B2 (enExample)
CN (1) CN108369199A (enExample)
DE (1) DE102015119267A1 (enExample)
ES (1) ES2865203T3 (enExample)
WO (1) WO2017081099A1 (enExample)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020054574A1 (ja) * 2018-09-10 2020-03-19 宇部興産株式会社 検査方法および検査装置
KR102802740B1 (ko) * 2019-05-30 2025-05-07 주식회사 엘지에너지솔루션 이차전지의 전극 내 수분 함량 분석을 위한 방법 및 시스템
CN111624234A (zh) * 2020-06-20 2020-09-04 宋海峰 粮食烘干塔用在线测水设备
JP2024035409A (ja) * 2022-09-02 2024-03-14 株式会社リガク 熱分析装置
JP2024035408A (ja) * 2022-09-02 2024-03-14 株式会社リガク 熱分析装置

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JPS5694950U (enExample) 1979-12-21 1981-07-28
DD155115A1 (de) 1980-12-04 1982-05-12 Gerd Arnoldi Verfahren und vorrichtung zur bestimmung der feuchtigkeit von feststoffgemischen
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DE4001928C2 (de) * 1990-01-24 1994-02-17 Elba Werk Maschinen Gmbh & Co Vorrichtung zur Messung der Eigenfeuchte von Schüttstoffen, insbesondere zur Messung der Eigenfeuchte von Beton-Zuschlagstoffen
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JP3416121B2 (ja) * 2001-02-07 2003-06-16 日本たばこ産業株式会社 揮発性成分の抽出装置および抽出方法
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Also Published As

Publication number Publication date
CN108369199A (zh) 2018-08-03
EP3374763A1 (de) 2018-09-19
US20180328834A1 (en) 2018-11-15
JP6933655B2 (ja) 2021-09-08
DE102015119267A1 (de) 2017-05-11
ES2865203T3 (es) 2021-10-15
JP2018533028A (ja) 2018-11-08
US10852226B2 (en) 2020-12-01
WO2017081099A1 (de) 2017-05-18

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